Hydrochloric Acid → 2,6-Dichloro-2',3',4'-trimethoxy-6'-methyl-benzophenone

HRID 361966

反応式

HRID 361966 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH3:13])[CH:6]=[C:7]([O:11][CH3:12])[C:8]=1[O:9][CH3:10].CCCCCCCC.[Cl:22][C:23]1[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[C:24]=1[C:25](Cl)=[O:26].Cl>[Fe](Cl)(Cl)Cl.O.C(OC(=O)C)C>[Cl:22][C:23]1[CH:31]=[CH:30][CH:29]=[C:28]([Cl:32])[C:24]=1[C:25]([C:4]1[C:5]([CH3:13])=[CH:6][C:7]([O:11][CH3:12])=[C:8]([O:9][CH3:10])[C:3]=1[O:2][CH3:1])=[O:26]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 356OctaneHCID 783922,6-Dichlorobenzoyl chlorideHCID 809223,4,5-Trimethoxytoluene

生成物 1

HCID 227199532,6-Dichloro-2',3',4'-trimethoxy-6'-methyl-benzophenone

試薬・触媒・溶媒 3

HCID 24380Iron chloride (FeCl3)触媒HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
105 °C

実験手順

A mixture of 3,4,5-trimethoxytoluene (9.11 g; 50 mmol), octane (25 ml) and iron(III)chloride (50 mg) is stirred at 105° C., and percolating nitrogene 2,6-dichlorobenzoylchloride (12.04 g; 57.5 mmol) is added dropwise within 15 minutes. The mixture is kept at 105° C. and stirred for another 15 minutes. After cooling to 50° C. ethylacetate (50 ml) is added, the mixture shaken twice with 2N hydrochloric acid, once with water and dried. The ethylacetate is evaporated (70° C.) and the liquid cooled with stirring. At 50° C. petrolether (50 ml) is added. The white crystals formed are sucked off, washed with petrolether and dried. Yield 12.55 g (70.7%), mp. 92° C.

後処理

  1. additionis added dropwise within 15 minutes
  2. customis kept at 105° C.
  3. stirringstirred for another 15 minutes
  4. additionis added
  5. customdried
  6. customThe ethylacetate is evaporated (70° C.)
  7. temperaturethe liquid cooled
  8. stirringwith stirring
  9. additionAt 50° C. petrolether (50 ml) is added
  10. customThe white crystals formed
  11. washwashed with petrolether
  12. customdried

出典と根拠

ORDレコード
ord-6e7b4119066c40779be23be71e686774
出典データセット
uspto-grants-1999_02
特許番号
US05866722

関連ノート

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